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Indian Standard
CHLOROB'ENZENE - SPECIFICATION
( F}lst Revision)
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res 71.080.20
© BIS 2003
BUREAU OF INDIAN STANDARDS
M,ANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
February 2003 Price Group 2
Organic Chemicals (Miscellaneous) Including Aromatic Hydrocarbons Sectional Committee, PCD 9
FOREWORD
This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized
by the Organic Chemicals (Miscellaneous) Including Aromatic Hydrocarbons Sectional Committee had been
approved by the Petroleum, Coal and Related Products Division Council.
This standard was first published in 1969. Since then lot of changes have taken place in its technology and
usage. Therefore, the Committee responsible for formulation of this standard decided to revise the standard to
update it and align with the international standards.
A new requirement of purity and related impurities by GLC method has been incorporated besides requirement
of moisture in this revision.
Chlorobenzene, also known as monochlorobenzene, is primarily used as solvent and in manufacture of phenol,
aniline, drugs, preservatives, perfumes and other organic solvents/products. It is a good solvent for cellulose
and other resins and also a heat transfer medium. The solvent grade material should be free, as far as possible
from benzene and other higher chlorides.
Chlorobenzene is combustible and in case of fire involving it, water can be used successfully if applied in the
form of a fog or spray. Carbon dioxide and dry chemical extinguishers are effective on small fires.
Following International Standard exist on the subject:
ISO 1697 : 1977 'Chlorobenzene for industrial use - List of methods of test'
For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS 2 : 1960' Rules for rounding off numerical values (revised)'. The number of significant places retained in the
rounded off value should be the same as that of the specified value in this standard.
IS 5591 : 2003
Indian Standard
CHLOROBENZENE - SPECIFICATION
( First Revision)
1 SCOPE 4 REQUIREMENTS
This standard prescribes the requirements and the 4.1 Description
methods of sampling and test for chlorobenzene.
The material shall be a clear, colourless, transparent
2 REFERENCES and mobile liquid with penetrating characteristics
odour of almonds. It shall be free from dissolved water,
The following standards contain provisions which,
suspended matter and sediments.
through reference in this text, constitute provisions of
this standard. At the time of publication the editions 4.2 The material shall comply with the requirements
indicated were valid. All standards are subject to prescribed in Table L
revision and parties to agreements based on the
5 PRECAUTIONS IN STORING AND
standard are encouraged to investigate the possibility
HANDLING
of applying the most recent editions of the standard
indicated below: Chlorobenzene is combustible and will burn if it comes
in contact with an open flame and therefore should
IS No. Title
not be stored near highly flammable and dangerously
1070: 1992 Reagent grade water (third revision)
reactive materials. Open flames and smoking shall not
1260 (Part 1) : Pictorial marking for handling and
be allowed where it is stored or handled (see also
1973 labelling of goods: Part 1 Dangerous
Foreword and 6.2.1).
goods (first revision)
2362 : 1993 Determination of water by Karl 6 PACKING AND MARKING
Fischer method (second revision)
6.1 The material shall be packed, stored and
4730: 1994 Methods for determination of density
transported in galvanized or mild steel drums. All the
of liquids (first revision)
containers in which the material is packed shall be
5298 : 1983 Method for determination of
dry, clean and free from substances soluble in
distillation range and distillation
chlorobenzene.
yield (first revision)
8883 (Part 1) : Methods of sampling chemicals and 6.2 The material shall be supplied in accordance with
1978 chemical products: Part 1 General the marking and delivery instructions given by the
requirements and precautions purchaser.
8883 (Part 21 Methods of sampling of chemicals
6.2.1 The containers shall be marked with the symbol
Sec 2) : 1978 and chemical products: Part 2
in Fig. 3 of IS 1260 (Part 1) and the following words
Sampling equipment, Section 2 For
in capitals.
liquids
9190 : 1979 Methods for determination of acidity CAUTION: VAPOUR HARMFUL, FLAMMABLE,
KEEP IN COOL PLACE.
and alkalinity in halogenated organic
solvents and their admixture 6.2.2 Each container shall be marked with:
3 GRADES a) Name of the material;
b) Name ofthe manufacturer and his recognized
The material shall be of two grades, namely:
trade-mark, if any;
a) Grade 1 - Primarily intended for the
c) Batch number and/or date of manufacture; and
manufacture of pharmaceuticals; can also be
d) Net mass of the contents.
used as solvent, and
6.2.3 The container may also be marked with the
b) Grade 2 - Primarily intended for the
Standard Mark.
manufacture of phenols, aniline,
preservatives, perfumes and other organic 6.2.3.1 The use of the Standard Mark is governed by
products; and for use as solvent. the provisions of the Bureau ofI ndian Standards Act,
IS 5591 : 2003
J 986 and the Rules and Regulations made thereunder. 7.3 Criteria For Conformity
The details of conditions under which the licence for
7.3.1 For Individual Samples
the use of the Standard Mark may be granted to
manufactures or producers may be obtained from the The lot shall be declared as conforming to the
Bureau of Indian Standards. requirements of description and distillation yield, if
each of the test results of the individual samples
7 SAMPLING satisfies the corresponding requirements of the test.
7.1 Representative samples of the material shall be 7.3.2 Composite Sample
drawn as prescribed in IS 8883 (Part 1) and
For declaring the conformity of a lot to the
IS 8883 (Part 2/Sec 2).
requirements of all other characteristics tested on the
composite sample, the test results shall satisfy the
7.2 Tests
relevant requirements given in Table I.
7.2.1 Tests for description and distillation yield shall
be conducted on individual samples. 8 QUALITY OF REAGENTS
7.2.2 Tests for the remaining characteristics shall be Unless specified otherwise, pure chemicals and
conducted on the composite samples. distilled water (see IS 1070) shall be employed in tests.
NOTE - 'Pure chemicals' shall mean chemicals that do not
contain impurities which affect the results of analysis.
Table 1 Requirements for Chlorobenzene
(Clauses 4.2 and 7.3.2)
SI Characteristics Requirements Method of Test, Ref to
No. __,
r-----------~-----------~, r~------A~----
Grade I Grade 2 Annex of this IS No.
Standard
(I) (2) (3) (4) (5) (6)
i) Relative density at 27/2rC 1.1 00 to 1.1 05 1.097 to 1.110 4730
Ii) Distillation yield, the temperature 2 to 97 (with in range of 2 to 97 (with in range 5298
corrected to 760 mOl Hg pressure 0.6 °C which shall be of 1.0 °C which shall be
percent by volume, Mill 130.5 to 132.5 0c) 129.5 to 132.5 0c)
iii) Residue on evaporation, percent by 0.01 0.02 A
mass, Ma:r
iv) Acidity, ppm, Max 30 30 4.2.2 of 9190
v) Free chlorine To pass the test B
vi) Moisture, percent by mass, Max 0.05 0.1 2362
vii) Purity, percent by mass, Min 99.5 98.0 C
viii) Benzene, percent by mass, Max 0.2 1 C
ix) Other isomers, percent, Max 0.2 0.5 C
NOTE -- The correction factor for relative density is +0.001 for each degree Celsius fall in temperature and -0.001 for each degree
Celsius rise in temperature within the range 25-35°C.
2
IS 5591 : 2003
ANNEXA
[Table 1, Sl No. (iii)]
DETERMINATION OF RESIDUE ON EV APORAT ION
A-l APPARATUS A-3 CALCULATION
A-1.1 Basin - porcelain or silica. Residue on evaporation,
M x 100
percent by mass
VD
A-2 PROCEDURE
where
Evaporate 100 ml of the material, accurately weighed in
M mass in g of the residue,
the tared basin over a steam-bath till dryness. Wipe the
bottom and dry the residue in an air-oven at 130 ± 2°C V volume of the material taken for test, and
for half an hour. Cool in a desiccator and weigh. D relative density of the material.
ANNEXB
[Table 1, Sl No. (v)]
TEST FOR FREE CHLORINE
8-0 OUTL1NE OF THE METHOD phthidine in 50 rul of glacial acetic acid and dilute
rapidly to 200 ml. Store the solution in the dark.
The material is shaken with 3, 3' dimethylnaphthidine
solution and the colour developed, if any is noted. B-2 PROCEDURE
B-1 REAGENTS B-2.1 To 50 rul of the material contained in a
measuring cylinder, add 5 ml of the 3,3' dimethylna
8-1.1 Glacial Acetic Acid
phthidine solution and shake the cylinder for 30 s.
B-1.2 3. 3 -Dimethylnaphthidine Solution B-2.2 The material shall be regarded to have passed
the test if no pink colour is developed.
Dissolve 0.01 g of finely ground 3,3' -dimethylna-
3
IS 5591 : 2003
ANNEXC
[Table 1, Sl No. (vii), (viii) and Ox)]
DETERMINATION OF PURITY BY GLC METHOD
C-l OUTLINE OF THE METHOD w
~
A small amount of the material is introduced into a gas w
w z
liquid partition column. The various components that w
OJ
are volatile under the conditions oftest are vapourized ~ w~
and transported through the column by a carrier gas. :9r: 0to
0:::
The separated components are measured in the effluent 0 0
by a detector and recorded as a chromatogram. The Qa. :..:.cJ
()
chromatogram is interpreted by applying component eO C
E I
attenuation and detector response factors to the peak 0
areas, and the relative concentrations are determined 0cq)
~m .0.. ..
by relating the individual peak responses to the total
peak responses. A typical chromatogram has been given
in Fig. 1 for guidance only.
C-2 APPARATUS
Any gas chromatograph equipped with FID (Flame
Ionization Detector) and electronic integrator may be
used. The chromatographic conditions given here are
for guidance only.
Column 15 percent OV-IOI on
chromosorb W (A W) 80-100
FIG. 1 A TYPICAL CHROMATOGRAH OF CHLOROBENZENE
mesh
Length x O.D 3M x 4 mm Glass
C-5 CALCULATIONS
Temperature Column Oven 130°C
Peak areas are calculated either by the most commonly
Injection port 225°C
used triangular method or automated integration. The
Detector 225 °C
sum ofthe areas is equated to 100 percent, it is implied
Flow rate Carrier gas, Nitrogen (N2) that all substances have come out of the column and
20 mllMin
all substances have the same response factor, however,
H 30 mllMin this is not the case in truth due to response factor of
2
Air 300 mllMin detector. Yet this method of calculation is fairly
Chart speed 20 mm/Min accurate.
The integrator automatically calculates the area
C-3 REAGENTS
percent of each individual impurity as follows:
a) Benzene A.R;
b) A standard reference material of Area percent of 'X'---A- x -100-
chlorobenzene of known purity; and Area of all peaks
c) Sample of chlorobenzene with impurities
where
(m- and p-dichlorobenzene, benzene, etc, of
known concentration). A = area of component 'X'.
Area percent of each impurity when multiplied with
C-4 PROCEDURE
response factor will give the actual mass percent of
Set the gas chromatograph. Inject 0.2 JlI of sample the concerned impurity.
with the help of 5 JlI syringe. Allow chromatograph
Percent 'X' = Area percent of 'X' x Response factor
to develop. At the end of the run find out area
percentage of all the components. Assay (as chlorobenzene), 100 - (Sum of the al1
percent by mass impurities present).
A standard blend containing necessary impurities may
be injected into chromatographic system to verify the Therefore, Purity (assay) 100 - (Water + Total area
impurities present in sample. of chlorobenzene = of percent impurities).
4
